CN103572060B - A kind of method of gold recovering ion from the aqueous solution - Google Patents
A kind of method of gold recovering ion from the aqueous solution Download PDFInfo
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- CN103572060B CN103572060B CN201310610382.5A CN201310610382A CN103572060B CN 103572060 B CN103572060 B CN 103572060B CN 201310610382 A CN201310610382 A CN 201310610382A CN 103572060 B CN103572060 B CN 103572060B
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- 239000010931 gold Substances 0.000 title claims abstract description 65
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 59
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 13
- 241000894006 Bacteria Species 0.000 claims abstract description 40
- 239000000243 solution Substances 0.000 claims abstract description 36
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000002086 nanomaterial Substances 0.000 claims abstract description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000002500 ions Chemical class 0.000 claims abstract description 11
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 8
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 239000002131 composite material Substances 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims abstract description 3
- 239000006228 supernatant Substances 0.000 claims abstract description 3
- 230000000968 intestinal effect Effects 0.000 claims description 11
- 241000194108 Bacillus licheniformis Species 0.000 claims description 5
- 241000186660 Lactobacillus Species 0.000 claims description 4
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 4
- 238000012258 culturing Methods 0.000 claims description 2
- 229940039696 lactobacillus Drugs 0.000 claims description 2
- 244000005700 microbiome Species 0.000 abstract description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007423 decrease Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 241000416536 Euproctis pseudoconspersa Species 0.000 abstract description 2
- 235000011089 carbon dioxide Nutrition 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- -1 gold ion Chemical class 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 230000001580 bacterial effect Effects 0.000 description 8
- 230000009514 concussion Effects 0.000 description 8
- 230000003534 oscillatory effect Effects 0.000 description 8
- 230000002829 reductive effect Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000282326 Felis catus Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001580017 Jana Species 0.000 description 1
- 241001518135 Shewanella algae Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- DAFYMZZLYPHPNG-UHFFFAOYSA-N gold;thiourea Chemical compound [Au].NC(N)=S DAFYMZZLYPHPNG-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Micro-Organisms Or Cultivation Processes Thereof (AREA)
Abstract
A method for gold recovering ion from the aqueous solution, relates to a kind of method of gold recovering ion.The method utilizing microorganism cells and the synergistic a kind of gold recovering ion from the aqueous solution of cetyl trimethylammonium bromide is provided.1) bacterium mud is dry, it is for subsequent use that bacterium powder is made in grinding; 2) in chlorauric acid solution, add the bacterium powder that step 1) obtains, add cetyl trimethylammonium bromide again, finally add ascorbic acid c, heating in water bath, vibration, after reaction, obtain the composite precipitation thing containing microbe and gold nano-material bottom reaction soln, directly pour out supernatant liquor, or centrifugation, obtain the matrix material containing microbe and gold nano-material, obtain elemental gold after high temperature sintering, gained elemental gold purity is higher.Organic efficiency is high, and microorganism cells consumption is low simultaneously, and follow-up roasting energy consumption is low, decreases the discharge of carbonic acid gas.
Description
Technical field
The present invention relates to a kind of method of gold recovering ion, especially relate to a kind of method of gold recovering ion from the aqueous solution.
Background technology
Gold, as one of most important precious metal, industrially has been widely used with tool in life.But the reserves of gold are limited, add that the market requirement of gold is growing, make the recycling of gold seem particularly important.The traditional methods such as chemical precipitation method, electrolytic process, ion exchange method, active carbon adsorption are for gold recovering from the aqueous solution, and compared with these traditional methods, biosorption process has lot of advantages, as high in processing efficiency; PH value and temperature range wide (pH3 ~ 9, temperature 4 ~ 90 DEG C) etc., thus biosorption technology has application prospect in gold recovery.Savvaidis etc. utilize the Gold Thiourea solution gold recovering (Biometals1998,11,145-151.) of a few class abandoned biomass; Nakajima etc. and Tsuruta etc. report master data (WorldJMicrobiolBiotetchnol2003,19, the 369-374. of numerous species microorganism cells in absorption and gold recovering; JGenApplMicrobiol2004,50,221-228.); Konishi etc. be reported in 25 DEG C, pH=7, hydrogen as under the condition of electron donor by precipitation gold (Hydrometallurgy2006,81,24-29.) in the reduction of anaeration in normal temperature bacterium Shewanella alga and cell; Macaskie etc. report under electron donor existence condition, to utilize microorganism cells absorbing and reducing method to reclaim gold (BiotechnolBioeng2007,96,631-639. in electron wastes; BiotechnolBioeng2008,99,1055-1064.; BiotechnolLett2010,32,1821-1828.).But the biosorption process based on microorganism is only applicable to the lower aqueous solution of gold ion concentration, and do not having under electron donor existence condition, the reduction process of gold ion is slower; Microorganism is comparatively limited to the loading capacity of gold ion, often uses microbial biomass to cause follow-up roasting process energy consumption high in a large number, produces a large amount of GHG carbon dioxide.
In recent years, the preparation of gold nano-material becomes one of study hotspot in field of nanometer technology.Utilize chemical reducing agent, be easy to the presoma of Au as HAuCl
4reduction, therefore pure chemistry reduction method is one of preparation method of the most frequently used gold nano-material.But; if be only that presoma and reductive agent react; the gold nano grain generated easily is reunited; and the controllability of nano particle pattern and granularity is poor; thus usually dispersion agent, protective material or diverting agent need be added; can not only agglomeration be reduced, regulating and controlling effect be played to Morphology and grain graininess simultaneously.Jana etc. adopt substep to add the method for crystal seed, with HAuCl at normal temperatures
4for presoma, ascorbic acid c(AA) be reductive agent, select cats product cetyl trimethylammonium bromide (CTAB), the relatively high nanowires of gold (JPhysChemB2001 of productive rate has been prepared in regulation and control, 105,4065-4067.), the method becomes the classical way that chemical method prepares gold nano-material, is that most investigator is used afterwards.But the method can only be used for the preparation of gold nano-material, and cannot be used for the recovery of gold ion in the aqueous solution.
Summary of the invention
Object of the present invention aims to provide the method utilizing microorganism cells and the synergistic a kind of gold recovering ion from the aqueous solution of cetyl trimethylammonium bromide (CTAB).
The present invention includes following steps:
1) bacterium mud is dry, it is for subsequent use that bacterium powder is made in grinding;
2) in chlorauric acid solution, add the bacterium powder that step 1) obtains, add cetyl trimethylammonium bromide (CTAB) again, finally add ascorbic acid c(AA), heating in water bath, vibration, after reaction, obtain the composite precipitation thing containing microbe and gold nano-material bottom reaction soln, directly pour out supernatant liquor, or centrifugation, obtain the matrix material containing microbe and gold nano-material, obtain elemental gold after high temperature sintering, gained elemental gold purity is higher.
In step 1), described bacterium mud can adopt the one in intestinal bacteria bacterium mud, lactobacillus bacterium mud, black-koji mould bacterium mud, S. cervisiae bacterium mud, Bacillus licheniformis mud etc.; Intestinal bacteria, lactobacillus, black-koji mould, S. cervisiae, Bacillus licheniformis are preferably through enlarged culturing.
In step 2) in, the volumetric molar concentration of described chlorauric acid solution can be 0.1 ~ 2.0mM, and the add-on of bacterium powder can be 0.005 ~ 0.05g; After adding CTAB again, in solution, the concentration of CTAB can be 2.5 ~ 10.0mM; Finally add ascorbic acid c(AA), make the concentration of AA in solution can be 0.25 ~ 2.0mM; At the temperature of described heating in water bath can be 30 ~ 90 DEG C, the time of described reaction can be 2 ~ 24h.
The present invention is under microorganism cells and CTAB synergy, ascorbic acid c(AA) fast restore gold ion the gold nano-material that height of formation is intensive around microorganism cells (nano wire, nano belt etc. are wound around microorganism cells), the matrix material that gold nano-material and microorganism cells are formed afterwards precipitates automatically, thus being coupled of realization response and sepn process, organic efficiency is high, microorganism cells consumption is low simultaneously, and follow-up roasting energy consumption is low, decreases the discharge of carbonic acid gas.In the present invention microorganism cells and CTAB indispensable, if only use microorganism cells, then gold enrichment capacity low; If only use CTAB, then cannot realize the recovery of gold.To present invention utilizes on microorganism cells abundant organo-functional group to interact with gold ion, be aided with the guide function of CTAB, introducing AA gold ion is reduced and the gold nano-material that height of formation is intensive around thalline as nanowires of gold, gold nano band etc.The recovery aspect of the present invention's gold ion is in aqueous expected to have a good application prospect.
Accompanying drawing explanation
Fig. 1 is SEM figure (scale is 100 μm) of gold nano-material prepared by embodiment 1.
Fig. 2 is SEM figure (scale is 2 μm) of gold nano-material prepared by embodiment 1.
Fig. 3 is the XRD figure spectrum of gold nano-material prepared by embodiment 1.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1:
In 10mL, 0.50mM chlorauric acid solution, add intestinal bacteria bacterium powder, do not have considerable change before reaction with after reaction 2h, bacterium powder is deposited on bottom.If first add CTAB(5.0mM in chlorauric acid solution), and then add bacterium powder or add CTAB after first adding bacterium powder, find that solution colour all manifests yellow, but the solution colour adding CTAB is darker.The flavescence of solution colour may with CTA+, complexing to occur relevant with Au (III), because addition sequence causes the change of Au in solution (III) concentration.First add bacterium powder, because adsorption makes Au (III) concentration decline rapidly, cause solution colour more shallow.Along with the lengthening of time, gold ion is reduced by phage surface group, and Au (III) concentration constantly reduces, and color is thin out gradually, does not have clustering phenomena to produce, and illustrates that gold nano grain is adsorbed on around thalline or solution inside in conjunction with Fig. 1 and 2.If add reductive agent AA(0.50mM), solution becomes bluish voilet immediately, and has particle to be suspended in solution inside, and after reaction 2h, solution colour shoals, and has particle to suspend in solution.It should be noted that when adding CTAB and AA by different order, produce a large amount of black particle soon, and reunite together.After reaction 24h, get upper solution respectively to detect through ultraviolet-visible, nanometer gold characteristic peak is there is not near 530nm, detect through AAS simultaneously, its Abs value is close to 0, this illustrates that in solution, Au (III) transforms by thalline absorbing and reducing substantially completely, occurs assemble and deposit.The XRD figure spectrum of gold nano-material prepared by embodiment 1 is see Fig. 3.
Embodiment 2:
Adopt intestinal bacteria dry bacterial powders, get 50 μ L chlorauric acid solutions (0.04856M) and be dissolved in and fill in the 50mL fine taper bottle of 10mL deionized water, add bacterium powder (0.005g), concussion, shakes up.250 μ LCTAB (0.1M) again, concussion is to being uniformly dispersed.Be placed in 30 DEG C of shaking bath (150r/min) oscillatory reaction 10min, then add 50 μ LAA (0.1M), shake to water white transparency.Continue to be placed in 30 DEG C of shaking bath (150r/min) oscillatory reaction 24h.
Embodiment 3 ~ 6
Adopt the intestinal bacteria dry bacterial powder in embodiment 2, hydrochloro-auric acid (HAuCl in reaction system
4) solution, bacteria suspension, AA solution concentration be fixed as 0.25mM, 0.5g/L and 0.50mM respectively, change the concentration (see table 1) of CTAB, repeat the preparation procedure identical with embodiment 2.
Table 1
Embodiment 7 ~ 9
Adopt the intestinal bacteria dry bacterial powder in embodiment 2, hydrochloro-auric acid (HAuCl in reaction system
4) solution, bacteria suspension concentration, CTAB solution concentration be fixed as 0.25mM, 0.5g/L and 5.0mM respectively, change the concentration (see table 2) of AA, repeat the preparation procedure identical with embodiment 2.
Table 2
Embodiment 10 ~ 11
Adopt the intestinal bacteria dry bacterial powder in embodiment 2, hydrochloro-auric acid (HAuCl in reaction system
4) solution, CTAB concentration, AA solution concentration be fixed as 0.25mM, 5.0mM and 0.50mM respectively, change the concentration (see table 3) of bacteria suspension, repeat the preparation procedure identical with embodiment 2.
Table 3
Embodiment 12 ~ 16
Adopt the intestinal bacteria dry bacterial powder in embodiment 2, in reaction system, the concentration of bacteria suspension, CTAB concentration, AA solution is fixed as 0.25mM, 5.0mM and 0.50mM respectively, changes HAuCl
4the concentration (see table 4) of solution, repeats the preparation procedure identical with embodiment 2.
Table 4
Embodiment 17:
Adopt black-koji mould dry bacterial powder, get 50 μ L chlorauric acid solutions (0.04856M) and be dissolved in and fill in the 50mL fine taper bottle of 10mL deionized water, add 250 μ LCTAB (0.1M), concussion, shakes up.Add bacterium powder (0.005g) again, concussion is to being uniformly dispersed.Be placed in 30 DEG C of shaking bath (150r/min) oscillatory reaction 30min, then add 50 μ LAA (0.1M), shake to water white transparency.Continue to be placed in 30 DEG C of shaking bath (150r/min) oscillatory reaction 24h.All the other preparation methods are with embodiment 2.
Embodiment 18:
Adopt Bacillus licheniformis dry bacterial powder, get 50 μ L chlorauric acid solutions (0.04856M) and be dissolved in and fill in the 50mL fine taper bottle of 10mL deionized water, add 250 μ LCTAB (0.1M), concussion, shakes up.Add bacterium powder (0.005g) again, concussion is to being uniformly dispersed.Be placed in 30 DEG C of shaking bath (150r/min) oscillatory reaction 30min, then add 50 μ LAA (0.1M), shake to water white transparency.Continue to be placed in 30 DEG C of shaking bath (150r/min) oscillatory reaction 24h.All the other preparation methods are with embodiment 2.
Embodiment 19:
Adopt intestinal bacteria dry bacterial powders, get 50 μ L chlorauric acid solutions (0.04856M) and be dissolved in and fill in the 50mL fine taper bottle of 10mL deionized water, add bacterium powder (0.005g), concussion, shakes up.Add 250 μ LCTAB (0.1M) again, concussion is to being uniformly dispersed.Be placed in 30 DEG C of shaking bath (150r/min) oscillatory reaction 10min, then add 50 μ LAA (0.1M), shake to water white transparency.Continue to be placed in 30 DEG C of shaking bath (150r/min) oscillatory reaction 24h.
Claims (4)
1. the method for gold recovering ion from the aqueous solution, is characterized in that comprising the following steps:
1) bacterium mud is dry, it is for subsequent use that bacterium powder is made in grinding; Described bacterium mud adopts the one in intestinal bacteria bacterium mud, lactobacillus bacterium mud, black-koji mould bacterium mud, S. cervisiae bacterium mud, Bacillus licheniformis mud;
2) in chlorauric acid solution, step 1 is added) the bacterium powder that obtains, add cetyl trimethylammonium bromide again, finally add ascorbic acid c, heating in water bath, vibration, after reaction, obtain the composite precipitation thing containing microbe and gold nano-material bottom reaction soln, directly pour out supernatant liquor, or centrifugation, obtain the matrix material containing microbe and gold nano-material, after high temperature sintering, obtain elemental gold; The add-on of described bacterium powder is 0.005 ~ 0.05g; The volumetric molar concentration of described chlorauric acid solution is 0.1 ~ 2.0mM/L; After adding cetyl trimethylammonium bromide, in solution, the concentration of cetyl trimethylammonium bromide is 2.5 ~ 10.0mM/L; After adding ascorbic acid c, in solution, the concentration of ascorbic acid c is 0.25 ~ 2.0mM/L.
2. the method for a kind of gold recovering ion from the aqueous solution as claimed in claim 1, is characterized in that in step 1) in, described intestinal bacteria, lactobacillus, black-koji mould, S. cervisiae, Bacillus licheniformis are through enlarged culturing.
3. the method for a kind of gold recovering ion from the aqueous solution as claimed in claim 1, is characterized in that in step 2) in, the temperature of described heating in water bath is 30 ~ 90 DEG C.
4. the method for a kind of gold recovering ion from the aqueous solution as claimed in claim 1, is characterized in that in step 2) in, the time of described reaction is 2 ~ 24h.
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| CN1736637A (en) * | 2005-09-09 | 2006-02-22 | 吉林大学 | Preparation method of monodisperse gold nanometer particle for immunological chromatography test |
| CN1817523A (en) * | 2006-01-05 | 2006-08-16 | 吉林大学 | Water-phase production of length controllable dendritic golden nanometer particle |
| KR20080069058A (en) * | 2007-01-22 | 2008-07-25 | 한국생명공학연구원 | Sythesis of gold nanoparticles of various crystal shapes using halide ion |
| CN101342599A (en) * | 2008-08-15 | 2009-01-14 | 厦门大学 | Method for preparing single-layer protection golden nano-particle |
| CN101705359A (en) * | 2009-11-10 | 2010-05-12 | 南京信息工程大学 | Method for recovering silver in silver-containing waste water by biological method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1736637A (en) * | 2005-09-09 | 2006-02-22 | 吉林大学 | Preparation method of monodisperse gold nanometer particle for immunological chromatography test |
| CN1817523A (en) * | 2006-01-05 | 2006-08-16 | 吉林大学 | Water-phase production of length controllable dendritic golden nanometer particle |
| KR20080069058A (en) * | 2007-01-22 | 2008-07-25 | 한국생명공학연구원 | Sythesis of gold nanoparticles of various crystal shapes using halide ion |
| CN101342599A (en) * | 2008-08-15 | 2009-01-14 | 厦门大学 | Method for preparing single-layer protection golden nano-particle |
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